#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:48:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179307 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/04/4320479.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4320479
loop_
_publ_author_name
'Savariraj Kingsley'
'Vadapalli Chandrasekhar'
'Christopher D. Incarvito'
'Matthew K. Lam'
'Arnold L. Rheingold'
_publ_contact_author
;
       Chandrasekhar. V
       Department of Chemistry
       IIT, Kanpur 208 016
       India
;
_publ_contact_author_email       vc@iitk.ac.in
_publ_contact_author_fax         '+91 512 597 436'
_publ_contact_author_phone       '+91 512 597 617'
_publ_section_title
;
 Tethered Pyrazolyl Phosphinate: Pyrazolyl-N- and Phosphoryl-O-Metal
 Coordination in Ph2P(O){OCH2CH2(3,5-Me2Pz)}
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5890
_journal_page_last               5896
_journal_paper_doi               10.1021/ic010454c
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C19 H21 Cl2 N2 O2 P Zn'
_chemical_formula_sum            'C19 H21 Cl2 N2 O2 P Zn'
_chemical_formula_weight         476.64
_chemical_melting_point          240
_chemical_name_common            PolyZn(4)
_chemical_name_systematic
;

   ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.5162(80)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7530(20)
_cell_length_b                   18.0247(20)
_cell_length_c                   11.9998(20)
_cell_measurement_temperature    193(2)
_cell_volume                     2099.7(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.1777
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9700
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    1.517
_exptl_absorpt_correction_T_max  0.8044
_exptl_absorpt_correction_T_min  0.6188
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.296
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.296
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1667
_reflns_number_gt                4103
_reflns_number_total             4533
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010454c_4.cif
_cod_data_source_block           PolyZn
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2099.75(3)
_cod_database_code               4320479
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 1.19804(4) 0.28819(2) -0.50473(3) 0.002(1) Uani 1 1 d . . .
Cl1 Cl 1.0018(1) 0.28373(6) -0.42562(9) 0.0040(1) Uani 1 1 d . . .
Cl2 Cl 1.1943(1) 0.36633(5) -0.64847(7) 0.0038(1) Uani 1 1 d . . .
P1 P 1.3997(1) 0.38225(5) -0.30881(6) 0.0023(1) Uani 1 1 d . . .
N1 N 1.2703(3) 0.1835(2) -0.5309(2) 0.0024(1) Uani 1 1 d . . .
O1 O 1.3359(2) 0.3225(2) -0.3832(2) 0.0030(1) Uani 1 1 d . . .
O2 O 1.5628(2) 0.3764(1) -0.2950(2) 0.0026(1) Uani 1 1 d . . .
N2 N 1.2982(3) 0.1514(2) -0.6308(2) 0.0024(1) Uani 1 1 d . . .
C1 C 1.2980(4) 0.1306(2) -0.4532(3) 0.0029(1) Uani 1 1 d . . .
C2 C 1.3410(4) 0.0657(2) -0.5030(3) 0.0035(1) Uani 1 1 d . . .
H2B H 1.3655 0.0202 -0.4664 0.0042 Uiso 1 1 calc R . .
C3 C 1.3410(3) 0.0805(2) -0.6149(3) 0.0031(1) Uani 1 1 d . . .
C4 C 1.2809(5) 0.1437(3) -0.3322(3) 0.0044(1) Uani 1 1 d . . .
H4A H 1.2497 0.1947 -0.3220 0.0066 Uiso 1 1 calc R . .
H4B H 1.3693 0.1359 -0.2876 0.0066 Uiso 1 1 calc R . .
H4C H 1.2126 0.1089 -0.3077 0.0066 Uiso 1 1 calc R . .
C5 C 1.3819(4) 0.0332(3) -0.7084(4) 0.0045(1) Uani 1 1 d . . .
H5A H 1.3696 0.0612 -0.7786 0.0067 Uiso 1 1 calc R . .
H5B H 1.3242 -0.0114 -0.7147 0.0067 Uiso 1 1 calc R . .
H5C H 1.4788 0.0188 -0.6931 0.0067 Uiso 1 1 calc R . .
C6 C 1.2703(4) 0.1910(2) -0.7359(3) 0.0029(1) Uani 1 1 d . . .
H6A H 1.3147 0.1644 -0.7951 0.0035 Uiso 1 1 calc R . .
H6B H 1.3114 0.2411 -0.7283 0.0035 Uiso 1 1 calc R . .
C7 C 1.1180(4) 0.1981(2) -0.7711(3) 0.0030(1) Uani 1 1 d . . .
H7A H 1.0710 0.2213 -0.7105 0.0036 Uiso 1 1 calc R . .
H7B H 1.1029 0.2296 -0.8387 0.0036 Uiso 1 1 calc R . .
C8 C 1.2297(4) 0.4903(2) -0.4012(3) 0.0034(1) Unai 1 1 d . . .
H8A H 1.1605 0.4533 -0.4003 0.0041 Uiso 1 1 calc R . .
C9 C 1.1951(4) 0.5599(2) -0.4421(3) 0.0039(1) Uani 1 1 d . . .
H9A H 1.1027 0.5707 -0.4695 0.0046 Uiso 1 1 calc R . .
C10 C 1.2956(5) 0.6141(2) -0.4432(3) 0.0040(1) Unai 1 1 d . . .
H10A H 1.2719 0.6621 -0.4714 0.0048 Uiso 1 1 calc R . .
C11 C 1.4306(4) 0.5986(2) -0.4033(3) 0.0041(1) Uani 1 1 d . . .
H11A H 1.4989 0.6361 -0.4037 0.0049 Uiso 1 1 calc R . .
C12 C 1.4664(4) 0.5283(2) -0.3625(3) 0.0035(1) Uani 1 1 d . . .
H12A H 1.5592 0.5178 -0.3358 0.0042 Uiso 1 1 calc R . .
C13 C 1.3661(3) 0.4733(2) -0.3608(3) 0.0026(1) Uani 1 1 d . . .
C14 C 1.2188(4) 0.3398(2) -0.1560(3) 0.0035(1) Unai 1 1 d . . .
H14A H 1.1653 0.3183 -0.2181 0.0042 Uiso 1 1 calc R . .
C15 C 1.1733(5) 0.3369(3) -0.0492(4) 0.0043(1) Unai 1 1 d . . .
H15A H 1.0872 0.3147 -0.0387 0.0051 Uiso 1 1 calc R . .
C16 C 1.2534(5) 0.3664(3) 0.0406(3) 0.0049(1) Unai 1 1 d . . .
H16A H 1.2229 0.3636 0.1133 0.0059 Uiso 1 1 calc R . .
C17 C 1.3781(5) 0.4002(3) 0.0265(3) 0.0045(1) Uani 1 1 d . . .
H17A H 1.4322 0.4202 0.0895 0.0054 Uiso 1 1 calc R . .
C18 C 1.4245(4) 0.4051(2) -0.0784(3) 0.0035(1) Unai 1 1 d . . .
H18A H 1.5097 0.4287 -0.0880 0.0042 Uiso 1 1 calc R . .
C19 C 1.3445(4) 0.3749(2) -0.1707(3) 0.0028(1) Unai 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 N1 100.41(11) . . ?
O1 Zn1 Cl1 104.39(8) . . ?
N1 Zn1 Cl1 110.85(8) . . ?
O1 Zn1 Cl2 109.37(8) . . ?
N1 Zn1 Cl2 116.41(8) . . ?
Cl1 Zn1 Cl2 113.84(4) . . ?
O1 P1 O2 111.71(14) . . ?
O1 P1 C13 113.81(15) . . ?
O2 P1 C13 104.29(15) . . ?
O1 P1 C19 110.70(16) . . ?
O2 P1 C19 106.55(15) . . ?
C13 P1 C19 109.36(16) . . ?
C1 N1 N2 105.2(3) . . ?
C1 N1 Zn1 126.7(2) . . ?
N2 N1 Zn1 128.1(2) . . ?
P1 O1 Zn1 151.22(17) . . ?
C7 O2 P1 115.3(2) 4_666 . ?
C3 N2 N1 110.9(3) . . ?
C3 N2 C6 128.1(3) . . ?
N1 N2 C6 120.8(3) . . ?
N1 C1 C2 110.3(3) . . ?
N1 C1 C4 121.9(3) . . ?
C2 C1 C4 127.8(3) . . ?
C3 C2 C1 106.6(3) . . ?
N2 C3 C2 107.0(3) . . ?
N2 C3 C5 122.3(4) . . ?
C2 C3 C5 130.6(4) . . ?
N2 C6 C7 112.5(3) . . ?
O2 C7 C6 108.1(3) 4_565 . ?
C9 C8 C13 120.9(4) . . ?
C8 C9 C10 119.7(4) . . ?
C9 C10 C11 120.4(4) . . ?
C10 C11 C12 120.2(4) . . ?
C11 C12 C13 120.0(4) . . ?
C12 C13 C8 118.8(3) . . ?
C12 C13 P1 123.8(3) . . ?
C8 C13 P1 117.4(3) . . ?
C15 C14 C19 119.3(4) . . ?
C16 C15 C14 119.9(4) . . ?
C15 C16 C17 120.8(4) . . ?
C18 C17 C16 120.6(4) . . ?
C17 C18 C19 119.2(4) . . ?
C18 C19 C14 120.2(3) . . ?
C18 C19 P1 120.4(3) . . ?
C14 C19 P1 119.4(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.985(2) . ?
Zn1 N1 2.049(3) . ?
Zn1 Cl1 2.2183(10) . ?
Zn1 Cl2 2.2244(9) . ?
P1 O1 1.496(2) . ?
P1 O2 1.587(2) . ?
P1 C13 1.776(4) . ?
P1 C19 1.796(3) . ?
N1 C1 1.342(5) . ?
N1 N2 1.382(4) . ?
O2 C7 1.465(4) 4_666 ?
N2 C3 1.353(5) . ?
N2 C6 1.451(4) . ?
C1 C2 1.396(5) . ?
C1 C4 1.496(5) . ?
C2 C3 1.369(5) . ?
C3 C5 1.493(5) . ?
C6 C7 1.510(5) . ?
C7 O2 1.465(4) 4_565 ?
C8 C9 1.376(6) . ?
C8 C13 1.405(5) . ?
C9 C10 1.384(6) . ?
C10 C11 1.385(6) . ?
C11 C12 1.390(6) . ?
C12 C13 1.394(5) . ?
C14 C15 1.397(5) . ?
C14 C19 1.405(5) . ?
C15 C16 1.377(7) . ?
C16 C17 1.385(7) . ?
C17 C18 1.380(6) . ?
C18 C19 1.402(5) . ?
